CN106830010B - Methanol and ammonium chloride extraction equipment and extraction process in glycine production - Google Patents
Methanol and ammonium chloride extraction equipment and extraction process in glycine production Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to equipment and a process for recovering methanol and extracting ammonium chloride in glycine production. Heating the II-effect heater slowly; slowly introducing mother liquor after glycine centrifugation into a preheater to enable the temperature of materials to reach 40 ℃; the preheated material enters a first-stage evaporation concentration system consisting of an I-effect heater A, an I-effect evaporator, an I-effect heater B and an I-effect methanol Roots compressor; the materials extracted from the bottom of the first-effect evaporator are introduced into a secondary evaporation concentration system consisting of a second-effect heater, a second-effect evaporator and a second-effect methanol Roots compressor; and (3) after the saturated ammonium chloride solution in the II-effect evaporator enters a thickener for thickening, the feed liquid is put into a centrifuge for separating white ammonium chloride products. The new process has the advantages of high steam utilization rate, small equipment investment, innocuous mother liquor treatment, energy conservation and environmental protection, and is suitable for wide application in glycine industry.
Description
Technical Field
The invention belongs to the technical field of glycine production, and particularly relates to a novel process for recovering methanol and extracting ammonium chloride in glycine production.
Background
Currently, the domestic glycine production still adopts a relatively traditional chloroacetic acid ammonolysis method. As the solubility of glycine and ammonium chloride in the synthetic liquid is different in methanol, after the glycine is extracted by methanol and centrifugally separated, the obtained centrifugal mother liquid contains a large amount of methanol, ammonium chloride and water, and simultaneously contains a small amount of glycine, urotropine and molecular ammonia. Because the centrifugal mother liquor has the characteristics of mixing organic matters and inorganic matters, multiple pollutant types, large ammonia nitrogen content, easy decomposition of urotropine at high temperature and the like, the problems of domestic glycine enterprises are always plagued: and how to effectively extract the methanol and the ammonium chloride in the centrifugal mother solution, thereby thoroughly achieving clean production. There are three major difficulties in recovering methanol and ammonium chloride from the centrifugation mother liquor: (1) energy consumption problems; (2) equipment corrosion problems; (3) In the evaporation process, problems of sublimation of ammonium chloride, decomposition of urotropine serving as a catalyst, complex chemical reaction caused by high-temperature evaporation and the like all generate evaporation condensate water and centrifugate with high ammonia nitrogen and high COD, and environmental protection risks exist.
The invention discloses a method and equipment for recovering ammonium chloride from glycine mother liquor, which is disclosed in the publication No. CN103303942A, and mainly comprises the steps of separating 90-93% of methanol from mother liquor after glycine alcohol precipitation and centrifugation through a packed rectifying tower, concentrating the residual liquid of the rectifying tower at low temperature through a two-stage countercurrent evaporator and a flash evaporator under a vacuum state, continuously cooling and crystallizing the concentrated liquid, and finally thickening and centrifugally separating crystal liquid to obtain an ammonium chloride product. However, the method has the defects of high equipment requirement, high steam energy consumption, low product purity, environmental problems caused by evaporating condensed water and final mother liquor, and the like.
The invention discloses a method for recycling mother liquor in glycine production process by chloroacetic acid method, which is characterized in that concentrating, burning and crystallizing glycine mother liquor, adopting specific burning temperature and crystallization temperature, reducing ammonium chloride loss, enabling ammonium chloride recovery rate to be more than 95%, enabling ammonium chloride quality to be high, and enabling mother liquor to be subjected to harmless treatment. However, the incineration temperature is 700-1000 ℃ and the crystallization temperature is 300 ℃, the energy consumption of the fuel used for heating is high, and the operation cost is high.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a new process for recovering methanol and extracting ammonium chloride in glycine production, which achieves the purposes of saving energy, reducing consumption, carrying out harmless treatment on mother liquor, reducing equipment failure rate, reducing maintenance and operation cost and thoroughly solving the environmental protection problem.
The invention mainly uses glycine mother liquor containing methanol and ammonium chloride to pass through a double-effect low-temperature evaporation concentration system which provides a heat source under the action of a Roots compressor, and obtains the ammonium chloride through continuous crystallization and separation, and meanwhile, the methanol solution can be continuously recovered without a rectification device, and the invention comprises the following steps:
the methanol and ammonium chloride extraction equipment in glycine production is characterized in that a conveying pipe is connected with a preheater through a feed pump, the top of the preheater is connected with an I-effect heater A, the I-effect heater A is connected with an I-effect evaporator, the bottom of the I-effect evaporator is connected with an I-effect heater B, and the bottom of the I-effect heater B is connected with the I-effect heater A through a circulating pump to form circulation;
the lower part of the I-effect heater A, I-effect heater B is connected with a methanol discharging tank through a conveying pipe;
the bottom of the I-effect evaporator is connected with a material transfer tank through a material transfer pipe, the material transfer tank is connected with a II-effect heater through a material transfer pump, and the II-effect heater is connected with the II-effect evaporator;
the bottom of the II-effect evaporator is connected with a thickener, and the thickener is connected with a centrifugal machine and then connected with a mother liquor pond.
The top of the I-effect evaporator is connected with an I-effect Roots methanol compressor, the I-effect Roots methanol compressor is respectively connected with an I-effect heater A, I-effect heater B through an oxygen online analyzer, and a methanol discharge tank is connected with the I-effect Roots methanol compressor through a methanol discharge pump to form a circulation system.
The lower part of the II-effect evaporator is connected with a forced circulation pump through a material conveying pipe, the forced circulation pump is connected with a II-effect heater, and the II-effect heater is connected with the II-effect evaporator; the mother liquor pond is connected with the forced circulation pump through the mother liquor reflux pump.
The top of the II-effect evaporator is connected with the II-effect Roots methanol compressor, the II-effect Roots methanol compressor is divided into two paths, one path is respectively connected with the I-effect heater A, I-effect heater B, the other path is connected with the condenser, the condenser is connected with the dilute methanol tank, and the methanol discharge tank is connected with the II-effect Roots methanol compressor through the methanol discharge pump to form a circulation system.
A method for extracting methanol and ammonium chloride in glycine production comprises the following steps:
(1) Firstly, introducing raw steam into the II-effect heater, regulating steam flow, and controlling the temperature of the preheater.
(2) The mother liquor after centrifugally separating glycine is heated to 30-40 ℃ by a preheater, and the heat source medium secondarily utilizes the latent heat of condensed water generated by steam generated in the II-effect heater.
(3) The preheated material passes through a primary evaporation concentration system consisting of an I-effect heater A, an I-effect evaporator and an I-effect heater B, and the vacuum degree in the system is kept at-0.07 Mpa.
(4) Under the vacuum condition, the methanol solution is gasified into methanol steam with the temperature of about 50-60 ℃ in the I-effect evaporator, the methanol steam is increased to 60-70 ℃ by utilizing the I-effect Roots methanol compressor, and the methanol steam after temperature increase enters the shell side of the I-effect heater A and the I-effect heater B to be reused. The system monitors the oxygen content in real time by using an oxygen online analyzer, and prevents the system from generating safety accidents due to incomplete nitrogen replacement or air entering in the operation process.
(5) The shell side condensate of the I effect heater A and the I effect heater B can be prepared into about 92% methanol solution, and 90% volume methanol solution in mother solution after the glycine is centrifugally separated is effectively separated.
(6) The solution containing a large amount of ammonium chloride is extracted from the bottom of the effect-I evaporator and enters a secondary evaporation concentration system consisting of an effect-II heater and the effect-II evaporator, the vacuum degree in the system is kept at-0.07 Mpa, and the effect-II heater adopts raw steam to provide an original heat source.
(7) The aqueous solution of methanol is vaporized into mixed steam of methanol and water with the temperature of about 80-85 ℃ in an II-effect evaporator under the vacuum condition, the methanol steam is increased to 90-95 ℃ by utilizing an II-effect Roots methanol compressor, and part of the methanol steam after temperature increase is parallel to the shell passes of an I-effect heater A and an I-effect heater B for secondary utilization and is used as heat supplement, and the other part of the methanol steam enters a condenser for condensation to obtain the methanol washing solution. Thus, the methanol and the water are effectively separated from the mother solution after the glycine is centrifuged.
(8) And (3) feeding the saturated ammonium chloride solution at the temperature of about 80 ℃ in the II-effect evaporator into a thickener for thickening, and then feeding the feed liquid into a centrifuge for separating an ammonium chloride product. So far, glycine centrifugal mother liquor is effectively treated.
In the system, the temperature and pressure systems are as follows:
currently, the glycine industry aims at mother liquor treatment after centrifugal separation of glycine, generally adopts a rectifying tower to separate methanol, and then carries out double-effect low-temperature evaporation on residual liquid of the rectifying tower to recover ammonium chloride. Compared with the method, the method has the following advantages:
(1) The whole process has higher steam utilization rate and lower steam energy consumption, and only a large amount of generated steam is needed in the heating stage of the initial II-effect heater in the starting process, and other equipment adopts material steam to provide a heat source.
(2) The system has low requirements on equipment and pipelines, does not relate to large rectifying tower equipment, and has low equipment investment.
(3) The concentration of the methanol can be accurately adjusted according to the actual production requirement.
(4) The oxygen online analyzer monitors the oxygen content in real time, prevents incomplete nitrogen replacement of the system or air entering in the running process, and has high safety coefficient.
(5) The mother liquor can achieve innocent treatment, can not produce white water with high ammonia nitrogen and high COD, can not produce red wastewater after ammonium chloride separation, and can achieve green production.
(6) Because the temperature in the evaporation process in the system is lower than 80 ℃, complex reactions among organic matters can not occur, COD, chromaticity and viscosity of the feed liquid can not be greatly increased, and the treatment difficulty is low.
(7) The ammonium chloride recovered by the process has high purity and good quality, can reach industrial grade white crystals, and can increase economic benefit.
(8) The process has the advantages of simple process and equipment and simple and convenient operation.
Drawings
FIG. 1 is a schematic diagram of a methanol and ammonium chloride extraction plant for glycine production, wherein 1. Feed pump, 2. Preheater, 3.I effect heater A,4.I effect heater B,5.I effect evaporator, 6.I effect Roots methanol compressor, 7. Oxygen on-line analyzer, 8. Methanol discharge tank, 9. Circulation pump, 10. Dilute methanol tank, 11. Transfer tank, 12. Condenser, 13. Transfer pump, 14.II effect heater, 15.II effect evaporator, 16.II effect Roots methanol compressor, 17. Forced circulation pump, 18. Mother liquor reflux pump, 19. Mother liquor pond, 20. Thickener, 21. Centrifuge.
Detailed Description
The specific implementation steps of the new process for recovering methanol and ammonium chloride are as follows:
example 1
Introducing raw steam into the II-effect heater, and regulating the steam flow to enable the temperature of the preheater to reach 40 ℃; slowly introducing mother liquor after glycine centrifugation into a preheater to enable the temperature of materials to reach 40 ℃; the preheated material enters a first-stage evaporation concentration system consisting of an I-effect heater A, an I-effect evaporator and an I-effect heater B, the vacuum degree at the top of the I-effect evaporator is kept at-0.07 Mpa, the temperature is kept at 60 ℃, and the temperature after the I-effect Roots methanol compressor is 70 ℃; introducing the materials extracted from the bottom of the first-effect evaporator into a secondary evaporation concentration system consisting of a second-effect heater and a second-effect evaporator, wherein the vacuum degree of the top of the second-effect evaporator is kept at-0.07 Mpa, the temperature is kept at 85 ℃, and the temperature after the second-effect Roots methanol compressor is 95 ℃; in the secondary evaporation process, methanol is continuously extracted, and the concentration is about 90-95%; and (3) after the saturated ammonium chloride solution at the temperature of about 80 ℃ in the II-effect evaporator enters a thickener for thickening, the feed liquid is put into a centrifuge for separating white ammonium chloride products, the purity of the ammonium chloride is 99.5%, and the recovery rate of the ammonium chloride is more than 98%.
Example 2
Introducing raw steam into the II-effect heater, and regulating the steam flow to enable the temperature of the preheater to reach 40 ℃; slowly introducing mother liquor after glycine centrifugation into a preheater to enable the temperature of materials to reach 40 ℃; the preheated material enters a first-stage evaporation concentration system consisting of an I-effect heater A, an I-effect evaporator and an I-effect heater B, the vacuum degree at the top of the I-effect evaporator is kept at-0.08 Mpa, the temperature is kept at 50 ℃, and the temperature after the I-effect Roots methanol compressor is 60 ℃; introducing the materials extracted from the bottom of the first-effect evaporator into a secondary evaporation concentration system consisting of a second-effect heater and a second-effect evaporator, wherein the vacuum degree of the top of the second-effect evaporator is kept at-0.08 Mpa, the temperature is kept at 80 ℃, and the temperature after the second-effect Roots methanol compressor is 90 ℃; in the secondary evaporation process, methanol is continuously extracted, and the concentration is about 90-95%; and (3) after the saturated ammonium chloride solution at the temperature of about 80 ℃ in the II-effect evaporator enters a thickener for thickening, the feed liquid is put into a centrifuge for separating white ammonium chloride products, and the purity of the ammonium chloride is 99.1%. The recovery rate of ammonium chloride is more than 97.5%.
Example 3
In glycine production, methanol and ammonium chloride extraction equipment is connected with a preheater 2 through a feed pump 1, the top of the preheater 2 is connected with an I-effect heater A3, the I-effect heater A3 is connected with an I-effect evaporator 5, the bottom of the I-effect evaporator 5 is connected with an I-effect heater B4, and the bottom of the I-effect heater B4 is connected with the I-effect heater A3 through a circulating pump 9 to form circulation;
the lower parts of the I-effect heater A3 and the I-effect heater B4 are connected with a methanol discharge tank 8 through a material conveying pipe;
the bottom of the I-effect evaporator 5 is connected with a material transfer tank 11 through a material transfer pipe, the material transfer tank 11 is connected with a II-effect heater 14 through a material transfer pump 13, and the II-effect heater 14 is connected with a II-effect evaporator 15;
the bottom of the II effect evaporator 15 is connected with a thickener 20, and the thickener 20 is connected with a centrifuge 21 and then is connected with a mother liquor pond 19.
The top of the I-effect evaporator 5 is connected with an I-effect Roots methanol compressor 6, the I-effect Roots methanol compressor 6 is respectively connected with an I-effect heater A3 and an I-effect heater B4 through an oxygen on-line analyzer 7, and a methanol discharge tank 8 is connected with the I-effect Roots methanol compressor 6 through a methanol discharge pump 22 to form a circulation system.
The lower part of the II-effect evaporator 15 is connected with a forced circulation pump 17 through a material conveying pipe, the forced circulation pump 17 is connected with a II-effect heater 14, and the II-effect heater 14 is connected with the II-effect evaporator 15; the mother liquor pond 19 is connected with the forced circulation pump 17 through a mother liquor reflux pump 18.
The top of the II-effect evaporator 15 is connected with the II-effect Roots methanol compressor 16, the II-effect Roots methanol compressor 16 is divided into two paths, one path is connected with the I-effect heater A3 and the I-effect heater B4 respectively, the other path is connected with the condenser 12, the condenser 12 is connected with the dilute methanol tank 10, and the methanol discharge tank 8 is connected with the II-effect Roots methanol compressor 16 through the methanol discharge pump 22 to form a circulation system.
Claims (10)
1. The methanol and ammonium chloride extraction equipment in glycine production is characterized in that a feed conveying pipe is connected with a preheater (2) through a feed pump (1), the top of the preheater (2) is connected with an I-effect heater A (3), the I-effect heater A (3) is connected with an I-effect evaporator (5), the bottom of the I-effect evaporator (5) is connected with an I-effect heater B (4), and the bottom of the I-effect heater B (4) is connected with the I-effect heater A (3) through a circulating pump (9) to form circulation;
the lower parts of the I-effect heater A (3) and the I-effect heater B (4) are connected with a methanol discharge tank (8) through a conveying pipe;
the bottom of the I-effect evaporator (5) is connected with a material transferring tank (11) through a material transferring pipe, the material transferring tank (11) is connected with a II-effect heater (14) through a material transferring pump (13), and the II-effect heater (14) is connected with a II-effect evaporator (15); the lower part of the II-effect evaporator (15) is connected with a forced circulation pump (17) through a conveying pipe, the forced circulation pump (17) is connected with a II-effect heater (14), and the II-effect heater (14) is connected with the II-effect evaporator (15);
the top of the II-effect evaporator (15) is connected through the II-effect Roots methanol compressor (16), the II-effect Roots methanol compressor (16) is divided into two paths, one path is connected with the I-effect heater A (3) and the I-effect heater B (4) respectively, the other path is connected with the condenser (12), the bottom of the II-effect evaporator (15) is connected with the thickener (20), and the thickener (20) is connected with the centrifugal machine (21) and then connected with the mother liquor tank (19).
2. The equipment for extracting methanol and ammonium chloride in glycine production according to claim 1, wherein the top of the I-effect evaporator (5) is connected with an I-effect Roots methanol compressor (6), the I-effect Roots methanol compressor (6) is respectively connected with an I-effect heater A (3) and an I-effect heater B (4) through an oxygen online analyzer (7), and a methanol discharge tank (8) is connected with the I-effect Roots methanol compressor (6) through a methanol discharge pump (22) to form a circulation system.
3. The equipment for extracting methanol and ammonium chloride in glycine production according to claim 1, characterized in that the mother liquor tank (19) is connected with the forced circulation pump (17) through a mother liquor reflux pump (18).
4. The methanol and ammonium chloride extraction device in glycine production according to claim 1, characterized in that the condenser (12) is connected with a dilute methanol tank (10), and the methanol discharge tank (8) is connected with a Roots methanol compressor (16) with II effect through a methanol discharge pump (22) to form a circulation system.
5. The extraction method of methanol and ammonium chloride in glycine production is characterized by comprising the following steps:
(1) The preheated material passes through a primary evaporation concentration system consisting of an I-effect heater A, an I-effect evaporator, an I-effect heater B and an I-effect Roots methanol compressor;
(2) After evaporation, the shell side condensate of the I-effect heater A and the I-effect heater B is prepared into 90-95% methanol solution, and at least 90% of the methanol solution in the mother solution after the centrifugal separation of glycine is effectively separated;
(3) The solution containing a large amount of ammonium chloride is extracted from the bottom of the effect I evaporator and enters a secondary evaporation concentration system consisting of an effect II heater and an effect II evaporator;
(4) After passing through the secondary evaporation concentration system, the saturated ammonium chloride solution at 80 ℃ in the II-effect evaporator enters a thickener for thickening, and the feed liquid is put into a centrifuge for separating ammonium chloride products.
6. The method for extracting methanol and ammonium chloride from glycine production of claim 5, wherein the preheated material is a material obtained by heating mother liquor after centrifugal separation of glycine to 30-40 ℃ through a preheater, and the temperature is obtained by introducing raw steam into an effect II heater, adjusting steam flow, controlling the temperature of the preheater to 30-40 ℃ and further adjusting the temperature of the material.
7. The method for extracting methanol and ammonium chloride from glycine as defined in claim 5, wherein the primary evaporation concentration system in step (1) maintains the vacuum degree within the range of-0.07 to-0.08 Mpa.
8. The method for extracting methanol and ammonium chloride from glycine as defined in claim 5, wherein the vacuum degree in the secondary evaporation concentration system in step (3) is maintained at-0.07 to-0.08 Mpa.
9. The method for extracting methanol and ammonium chloride from glycine production as defined in claim 5, wherein in the primary evaporation concentration system, the methanol solution is gasified into methanol vapor with the temperature of 50-60 ℃ in the I-effect evaporator, the I-effect Roots methanol compressor increases the temperature of the methanol vapor to 65-70 ℃, and the methanol vapor after temperature increase is parallel fed into the shell passes of the I-effect heater A and the I-effect heater B for secondary use.
10. The method for extracting methanol and ammonium chloride from glycine production as defined in claim 5, wherein in the secondary evaporation concentration system, aqueous solution of methanol is vaporized into mixed steam of methanol and water with temperature of 80-85 ℃ in an II-effect evaporator, the methanol steam is raised to 90-95 ℃ by utilizing an II-effect Roots methanol compressor, part of the methanol steam after temperature raising is parallel fed into shell passes of an I-effect heater A and an I-effect heater B for secondary utilization, and is used as heat supplement, and part of the methanol steam enters a condenser for condensation to obtain methanol washing solution.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108658374B (en) * | 2018-05-18 | 2021-06-08 | 湖北泰盛化工有限公司 | Clean treatment method of glycine production wastewater |
| CN108821944A (en) * | 2018-08-03 | 2018-11-16 | 上海飒环保工程科技有限公司 | A kind of comprehensive processing method of amion acetic acid centrifuge mother liquor |
| CN110980844A (en) * | 2019-11-22 | 2020-04-10 | 天津乐科节能科技有限公司 | Treatment method of glycine production wastewater |
| CN115215354A (en) * | 2021-04-21 | 2022-10-21 | 湖北泰盛化工有限公司 | Device and process for treating ammonium chloride waste liquid in industrial glycine production |
| CN115215394B (en) * | 2021-04-21 | 2023-05-02 | 湖北泰盛化工有限公司 | Treatment process of ammonium chloride waste liquid in glycine production |
| CN115286525A (en) * | 2022-09-30 | 2022-11-04 | 山东民基新材料科技有限公司 | Separation method of glycine and ammonium chloride mixed crystal solid |
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